HPLC法测定心脑脉舒口服液中阿魏酸含量

本文建立了心脑脉舒口服液中阿魏酸含量测定方法。色谱柱：ＹＷＧ－Ｃ１８，４．０×１５０ｍｍ；流动相：甲醇－水－冰乙酸（３３：６６：１）；流速：１．０ｍ１／ｍｉｎ；ＵＶ检测波长：３２０ｍｍ。结果表明，方法快速、准确、灵敏、重现性好。阿魏酸浓度在０．２～１．０μｇ／μ１范围内线性关系良好（γ＝０．９９９８），加样回收率为９６．７４％，ＲＳＤ＝２．７％，实际测定１０批样品结果满意。     

HPLC法测定人血清索他洛尔浓度

应用ＨＰＬＣ方法检测血清中索他洛尔浓度，以阿替洛尔为内标，采用Ｃ１８分析椎琢保护柱，流动相为甲醇：乙腈：ＰＢ。流速为１．０ｍｌ／ｍｉｎ。提取溶剂为三氯甲烷；异丙醇，采用荧光检测器，激光波长及发射波长分别为２３５ｎ，及３１３ｍｍ实验结果表明：索他洛尔与内标分离良好，保留时间分别为５ｍｉｎ一６．７ｍｉｎ，在血清中萃取的绝对回收率分别为８０．０％及８１．５％，索他洛尔在０－５μｇ／ｍｌ范围内线性关系良好     

固相萃取高效液相色谱法检测生物样本中甲氨喋呤

目的：建立生物样品中甲氨喋呤（ＭＴＸ）浓度测定方法。方法：固相萃取净化和富集样品,高效液相色谱法测定血清和脑脊液中ＭＴＸ含量。色谱条件：以Ｃ１８柱为分析柱,流动相为甲醇－乙腈－磷酸盐缓冲液（２：７：９１）,流带０．８ｍＬ．ｍｉｎ＾－１,柱温２５℃,检测波长３１３ｎｍ。结果：在０．０５￣８０μｇ．ｍＬ＾－１范围内呈线性,回收率为９０％以上,血清中ＭＴＸ最低检测限为１０ｎｇ．ｍＬ＾－１,脑脊液中最低检     

反相HPIC法测定血清布洛芬含量

本文以消炎痛为内标，用反相ＨＰＩＣ测定血清中的布洛芬。色谱柱为ＹＷＧＣ（１８）（１０μｍ）２００ｍｍ×５ｍｍ。流动相为甲醇－２０ｍｍｏｌ／Ｌ。磷酸二氢钾缓冲液（７０：３０，ｐＨ３．８）。流速为１ｍｌ／ｍｉｎ。检测波长为２２５ｎｍ。色谱柱柱温为５０℃。布洛芬和内标的保留时间分别为７．２和５．２ｍｉｎ。布洛芬的检测限为２ｎｇ（Ｓ／Ｎ≥４：１）。血清样品的预处理采用１：１的乙腈沉淀蛋白后直接进样。血清布洛芬浓度在０．５～６４μｇ／ｍｌ范围呈线性关系（ｒ＝０．９９９６）。天内天间精密度分别为１．６％～３．９％和２．１％～５．０％。     

反相高效液相色谱法测定人血浆中氨溴索浓度

目的：建立测定血浆中氨溴索浓度的反相高效液相色谱法。方法：血浆样品用乙醚提取,醚层经００１ｍｏｌ·Ｌ－１盐酸提取后进样,色谱柱为ＲｅｓｏｌｖｅＣ１８４６ｍｍ×２５０ｍｍ（５μｍ）,流动相为乙腈－甲醇－００１ｍｏｌ·Ｌ－１ｐＨ７０磷酸盐缓冲液－四氢呋喃（３５０∶３５０∶２７５∶２５）,流速１５ｍＬ·ｍｉｎ－１,检测波长２４２ｎｍ,外标法峰高定量。结果：本法最低检测浓度５ｎｇ·ｍＬ－１,线性范围１０～３２０ｎｇ·ｍＬ－１,回归方程为Ｈ＝２４５＋１６４Ｃ,ｒ＝０９９９５,日内ＲＳＤ为２７％～５３％,日间ＲＳＤ为３２％～８２％。结论：该法适用于盐酸氨溴索片的药代动力学研究。     

HPLC测定血清中阿昔洛韦浓度的方法改进

改良ＨＰＬＣ测定人及大鼠血清中阿昔洛韦浓度的分析方法。和Ｗａｔｅｒｓ高效液相色谱仪，＝ＢｏｎｄａｐａｋＣ１８柱，流动相为甲－水，流速１．５ｍＬ／ｍｉｎ，检测波长２５４ｎｍ，内标物为扑热息痛，血清样品采用甲醇去蛋白。阿昔洛韦血清浓度。０．０５－１．６ｍｇ／Ｌ范围内一峰高呈良好线性关系，大鼠和人血清中相对回收率分别为９３．３１％及９０．６９％；最低检测浓度均为０．０２５ｍｇ／Ｌ；天内精密度分别为０．８     

HPLC法测定两性霉素B含量

目的：用高效液相色谱法测定两性霉素 Ｂ含量。方法：外标法定量，色谱柱为μ－ Ｂｏｎｄａｐａｋ Ｃ柱（１０μｍ， ３．９ｍｍ × ３００ｍｍ）；流动相为乙腈－磷酸盐缓冲液（ｐＨ６． ２０）（５５： ４５， ｖ／ｖ），其中含 ０．０２ｍｏｌ／Ｌ四丁基溴化铵；流速１．２ｍｌ／ｍｉｎ；检测波长４０５ｎｍ。结果：两性霉素Ｂ浓度在３．０～２１．０μｇ／ｍｌ范围内线性关系良好，其相关系数 ｒ＝ ０．９９９７，本方法的平均回收率为 １０２．９４ ± ２．１７％，日内和日间相对标准偏差分别平均为 ２．８０％和５．２５％。结论：该方法简便、快速、准确、重现性好。     

HPLC法同时测定人血浆中地尔硫卓及其代谢产物

本法用ＷａｔｅｒｓＢａｓｅｌｉｎｅ８１０色谱工作站，Ｗａｔｅｒｓ径向加压柱（Ｎｏｖａ－ＰａｋＣ＿（１８）８ｍｍ×１０ｃｍ，４μｍ），检测波长ＵＶ２３８ｎｍ，流动相为甲醇－水－二氯甲烷－０．１ｍｏｌ／Ｌ醋酸铵（６４：２３．５：２．５：１０），流速：２．０ｍｌ／ｍｉｎ；血样用混合溶剂一次提取，地尔硫和去乙酰地尔硫的提取回收率分别为８５．２％、８２．３％，平均方法回收率分别为９９．６％、１０１．１％，最低检测浓度均为５ｎｇ／ｍｌ。     

HPLC法测定压平乐血药浓度及药代动力学研究

本文采用反相ＨＰＬＣ法测定压平乐健康人血清浓度，并对压平乐片的药动学进行了研究。色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ１８，４．６×１５０ｍｍ，流动相为甲醇－０．０２Ｍ磷酸氢二铵（９：１）。检测波长为２２７ｎｍ，流速０．５ｍｌ／ｍｉｎ。用ＰＫＢＰ－Ｎ１程序拟合血浓－时间曲线，结果符合一室模型，其半衰期为ｔ１／２＝７．２１±０．８９ｈ。     

高效液相色谱法分析组合化学合成结构相似小分子多肽

目的：为组合化学合成结构相似小分子多肽提供快速准确的ＨＰＬＣ分析方法。方法：ＰｅｓｏｌｖＣ１８柱（５μｍ，４．６ｍｍ＊２００ｍｍ）。流动相：乙腈－水（２０：８０），内含０．１％三氟乙酸为流动相酸性调节剂。检测波长：２１４ｎｍ。结果：目标多肽纯度范围２６．３６％～７７．０２％，迁移时间２．８９～３０．１５ｍｉｎ。７号多肽纯度和迁移时间的ＲＳＤ分别为１．９％和１．４％。结论：应用本方法可快速准确分离分     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.